CN113512661B - Diamond @ TiC enhanced high-strength conductive copper-based composite material and preparation method thereof - Google Patents
Diamond @ TiC enhanced high-strength conductive copper-based composite material and preparation method thereof Download PDFInfo
- Publication number
- CN113512661B CN113512661B CN202110441817.2A CN202110441817A CN113512661B CN 113512661 B CN113512661 B CN 113512661B CN 202110441817 A CN202110441817 A CN 202110441817A CN 113512661 B CN113512661 B CN 113512661B
- Authority
- CN
- China
- Prior art keywords
- diamond
- copper
- tic
- powder
- composite material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
Abstract
The invention discloses a diamond @ TiC enhanced high-strength conductive copper-based composite material and a preparation method thereof, wherein the copper-based composite material comprises a copper base and a diamond @ TiC reinforcement, wherein the diamond @ TiC reinforcement accounts for 5-50% of the total mass of the copper-based composite material, the diamond @ TiC reinforcement is core-shell structure diamond @ TiC with a TiC interface layer, the TiC is mutually connected to form a network-shaped framework, and a copper base body is distributed among the network-shaped TiC frameworks. The copper-based composite material has excellent electric conductivity and heat conductivity, and higher strength, hardness and wear resistance.
Description
Technical Field
The invention relates to the technical field of copper-based composite material processing, in particular to a diamond @ TiC enhanced high-strength conductive copper-based composite material and a preparation method thereof.
Background
The diamond has the characteristics of high melting point, high hardness, high elastic modulus and the like, and simultaneously has low thermal expansion coefficient (2.3 multiplied by 10)-6·K-1) And high thermal conductivity (about 2000 W.m)-1·K-1) And is a commonly used reinforcing phase for metal matrix composites. The diamond is compounded with copper with good electric and thermal conductivity to prepare the copper-based composite material, so that the strength, hardness and wear resistance of the copper alloy can be remarkably improved while the good electric and thermal conductivity of the copper alloy is maintained, the thermal expansion coefficient is reduced, and the copper-based composite material is improvedThe material has good heat-conducting property, and is an ideal material for manufacturing elements which require high strength, high electric conduction and high heat-conducting property, such as large-scale integrated circuit lead frames, electric contacts and the like. With the development of the artificial diamond industry in recent years, the price of the artificial diamond is remarkably reduced, and research and application of the artificial diamond in the field of composite materials are further promoted. For example, the thermal conductivity of 853 W.m is respectively prepared by the Beijing nonferrous metals research institute and the national defense science and technology university-1·K-1And 768 W.m-1·K-1The diamond reinforced copper-based composite material. In patent CN109930022A, a graphene/diamond mixed reinforced copper-based composite material and a preparation method thereof are disclosed, in the prepared composite material, graphene is uniformly adhered on the surface of diamond particles, the problem that two phases are difficult to be uniformly mixed is solved, and the interface combination of diamond and copper matrix and the interface combination of graphene and copper matrix are realized. In patent CN109930022A, a graphene/diamond mixed reinforced copper-based composite material and a preparation method thereof are disclosed, in the prepared composite material, graphene is uniformly adhered on the surface of diamond particles, the problem that two phases are difficult to be uniformly mixed is solved, and the interface combination of diamond and copper matrix and the interface combination of graphene and copper matrix are realized.
For the diamond reinforced copper-based composite material, because the wettability of diamond and copper is extremely poor, even at the high temperature of 1400 ℃, the contact angle between the diamond and the copper is still up to 128 degrees, and the diamond does not react with the copper, so that the interface bonding force between the diamond and the copper matrix in the composite material is poor, and how to improve the interface characteristic is a key problem in the preparation process of the diamond reinforced copper-based composite material. At present, modification treatment such as coating is carried out on the surface of diamond, and the coating and the diamond react to form an interface layer, which is a main means for improving the characteristics of the interface between the diamond and a copper matrix, for example, patent CN111519076 discloses a diamond particle reinforced metal matrix composite material, and a preparation method and application thereof. The patent CN11889676A discloses a method for preparing a diamond copper-based composite material by an additive manufacturing process, the invention plates a composite coating layer on the surface of diamond powder by a plating process, the composite coating layer is a carbide coating layer or a metal simple substance coating layer for improving the interface performance of diamond and a matrix, the outer coating layer is pure copper, and then the composite material with excellent performance is prepared by selective laser melting, hot isostatic pressing and other processes.
Currently, diamond-reinforced copper-based composites are mainly used as thermal management materials requiring high thermal conductivity, and their application in high-strength conductive composites is currently less. In fact, on one hand, high strength, hardness and wear resistance, as well as excellent heat conductivity and low thermal expansion coefficient are important performance indexes of the high-performance high-strength conductive composite material, so that the high-strength conductive copper-based composite material with excellent comprehensive performance can be prepared by taking diamond as a reinforcement.
Disclosure of Invention
The invention aims to prepare a high-performance high-strength conductive copper-based composite material by using diamond as a reinforcement body, and form a titanium carbide layer on the surface of the diamond through an interface reaction, so that the interface characteristic of the composite material is improved. The diamond @ TiC enhanced high-strength conductive copper-based composite material is characterized in that coating of a copper-titanium melt on diamond is achieved below a Ti-C reaction temperature by utilizing the characteristic that titanium and copper can react to form a low-melting-point eutectic structure, the diamond and the copper-titanium melt further react at a high temperature to form a TiC interface layer, generated TiC grows and is connected into a network shape by controlling parameters such as composite material components, sintering time and the like, and meanwhile, tissue densification is achieved through hot-pressing sintering, and the diamond enhanced copper-based composite material is prepared.
The diamond @ TiC enhanced high-strength conductive copper-based composite material comprises a copper base and diamond @ TiC reinforcements, wherein the diamond @ TiC reinforcements account for 5% -50% of the total mass of the copper-based composite material, the diamond @ TiC reinforcements are core-shell structure diamond @ TiC with TiC interface layers, the TiC reinforcements are mutually connected to form a network-shaped framework, and a copper base body is distributed among the network-shaped TiC frameworks.
The invention also provides a preparation method of the diamond @ TiC enhanced high-strength conductive copper-based composite material, which comprises the following steps of:
(1) preparing raw materials: weighing the following raw materials in percentage by mass:
0.45 to 35 percent of titanium powder,
4.55 to 40 percent of diamond powder,
the balance of copper powder;
wherein the mass ratio of the titanium powder to the diamond powder is 1:10-7: 2;
(2) mixing raw materials: firstly, dividing copper powder into two parts, then mixing titanium powder with a first part of copper powder, mixing and ball-milling for 1-10h in a planetary ball mill mixer, and uniformly mixing the mixed powder obtained by ball-milling with diamond powder and a second part of copper powder to obtain Cu-Ti-diamond mixed powder;
(3) hot-pressing and sintering: and sintering the Cu-Ti-diamond mixed powder in a hot pressing sintering furnace or a hot isostatic pressing sintering furnace under a certain atmosphere in a segmented manner, and cooling to obtain the finished copper-based composite material.
The invention adopts a two-step sintering method, controls the sintering temperature, the sintering pressure and the sintering time of two-step sintering respectively to ensure that titanium and diamond fully react to form TiC, and simultaneously realizes the densification of the structure.
Furthermore, in the step (1), the granularity of the titanium powder is 5-300 mu m, the purity is more than 99%, the degree of the diamond powder is 0.5-50 mu m, the purity is more than 99%, the granularity of the copper powder is 1-400 mu m, and the purity is more than 99%.
Further, the mass ratio of the titanium powder to the first part of copper powder in the step (2) is 1: 0.5-6.
Further, the step (3) is to perform sectional calcination on the Cu-Ti-diamond mixed powder under vacuum, inert gas or reducing atmosphere.
Further, in the step (3), the sintering temperature of the first stage is 800-
Compared with the prior art, the invention has the beneficial technical effects that:
(1) the TiC interface layer is synthesized through the self-generated reaction to form the core-shell structure diamond @ TiC reinforcement, so that the interface characteristic of diamond and a copper matrix is effectively improved;
(2) the TiC interface layers in the composite material prepared by the method are connected into a continuous network to form a reinforced framework of the composite material, and the copper matrix is distributed among the TiC frameworks and used as an excellent conductive phase, so that the composite material has excellent electric conductivity and heat conductivity, and higher strength, hardness and wear resistance.
Drawings
The invention is further illustrated in the following description with reference to the drawings.
FIG. 1 is a microstructure diagram of a diamond-reinforced high-strength conductive copper-based composite material prepared in example 1 of the present invention;
FIG. 2 is a deep-etched structure diagram of the diamond-reinforced high-strength conductive copper-based composite material prepared in example 1 of the present invention.
Detailed Description
The diamond @ TiC enhanced high-strength conductive copper-based composite material provided by the invention is further explained by combining with the embodiment
Example 1
(1) Preparing raw materials: weighing titanium powder with the granularity of 50 mu m and the purity of more than 99 percent according to the mass percent: 30 percent of diamond powder with the granularity of 5 mu m and the purity of more than 99 percent, and the balance of copper powder with the granularity of 200 mu m and the purity of more than 99.5 percent;
(2) preparing Cu-Ti-diamond mixed powder: firstly, mixing titanium powder with part of copper powder, wherein the mass ratio of the titanium powder to the copper powder is 1:1, vacuumizing and filling argon in a planet ball mill mixer, mixing and ball milling for 3 hours, and mechanically and uniformly mixing mixed powder obtained by ball milling with diamond powder and the rest copper powder to obtain the required Cu-Ti-diamond mixed powder;
(3) hot-pressing and sintering: and putting the mixed powder into a cylindrical mold, placing the cylindrical mold in a hot-pressing sintering furnace, carrying out hot-pressing sintering under the protection of argon, heating to 850 ℃ at the first stage, preserving heat for 1h under the pressure of 100MPa, then further raising the temperature to 1250 ℃, preserving heat for 2h under the pressure of 500MPa, and cooling to obtain the finished copper-based composite material.
The microstructure of the gold composite material prepared in this example is shown in fig. 1, and the texture of the etch back is shown in fig. 2. It can be seen from the figure that the composite material prepared in the embodiment has a compact structure, wherein the diamond is converted into core-shell structure diamond @ TiC with TiC as an interface layer, and the TiC interface layers are connected with each other to form a continuous network skeleton, so that the core-shell structure diamond @ TiC reinforced copper-based composite material is obtained.
The hardness of the TiC reinforced copper-based electric contact composite material prepared in the embodiment is 275HV, and the electric conductivity is 35% IACS.
Example 2
(1) Preparing raw materials: weighing titanium powder with the granularity of 100 mu m and the purity of more than 99 percent according to the mass percent: 15 percent of diamond powder with the granularity of 8 mu m and the purity of more than 99 percent, and the balance of copper powder with the granularity of 200 mu m and the purity of more than 99.5 percent;
(2) preparing Cu-Ti-diamond mixed powder: firstly, mixing titanium powder with part of copper powder, wherein the mass ratio of the titanium powder to the copper powder is 1: 3, vacuumizing and filling argon in a planetary ball mill mixer, mixing and ball-milling for 3 hours, and mechanically and uniformly mixing mixed powder obtained by ball-milling with diamond powder and the rest copper powder to obtain the required Cu-Ti-diamond mixed powder;
(3) hot-pressing and sintering: putting the mixed powder into a cylindrical mold, placing the cylindrical mold in a hot-pressing sintering furnace, carrying out hot-pressing sintering under the protection of argon, heating to 900 ℃ at the first stage, carrying out heat preservation for 1h under the pressure of 50MPa, then further raising the temperature to 1150 ℃, carrying out heat preservation for 3h under the pressure of 400MPa, and finally obtaining the composite material after cooling.
Through testing, the hardness of the TiC reinforced copper-based electric contact composite material prepared in the embodiment is 220HV, and the electric conductivity is 44% IACS.
Example 3
(1) Preparing raw materials: weighing titanium powder with the granularity of 50 mu m and the purity of more than 99 percent according to the mass percent: 10 percent of diamond powder with the granularity of 2 mu m and the purity of more than 99 percent, and the balance of copper powder with the granularity of 100 mu m and the purity of more than 99.5 percent;
(2) preparing Cu-Ti-diamond mixed powder: firstly, mixing titanium powder with part of copper powder, wherein the mass ratio of the titanium powder to the copper powder is 1: 4, vacuumizing and filling argon in a planet ball mill mixer, mixing and ball milling for 2 hours, and mechanically and uniformly mixing mixed powder obtained by ball milling with diamond powder and the rest copper powder to obtain the required Cu-Ti-diamond mixed powder;
(3) hot-pressing and sintering: putting the mixed powder into a cylindrical mold, placing the cylindrical mold in a hot-pressing sintering furnace, carrying out hot-pressing sintering under the protection of argon, heating to 900 ℃ at the first stage, carrying out heat preservation for 1h under the pressure of 100MPa, then further raising the temperature to 1250 ℃, carrying out heat preservation for 3h under the pressure of 500MPa, and finally obtaining the composite material after cooling.
Through testing, the hardness of the TiC reinforced copper-based electric contact composite material prepared in the embodiment is 170HV, and the electric conductivity is 56% IACS.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (3)
1. The diamond @ TiC enhanced high-strength conductive copper-based composite material is characterized by comprising a copper base and a diamond @ TiC reinforcement, wherein the diamond @ TiC reinforcement accounts for 5% -50% of the total mass of the copper-based composite material, the diamond @ TiC reinforcement is core-shell structure diamond @ TiC with a TiC interface layer, the TiC is mutually connected to form a network-shaped framework, and a copper base is distributed among the network-shaped TiC frameworks;
the preparation method of the diamond @ TiC enhanced high-strength conductive copper-based composite material comprises the following steps of:
(1) preparing raw materials: weighing the following raw materials in percentage by mass:
0.45 to 35 percent of titanium powder,
4.55 to 40 percent of diamond powder,
the balance of copper powder;
wherein the mass ratio of the titanium powder to the diamond powder is 1:10-7: 2;
(2) mixing raw materials: firstly, dividing copper powder into two parts, then mixing titanium powder with a first part of copper powder, mixing and ball-milling for 1-10h in a planetary ball mill mixer, and uniformly mixing the mixed powder obtained by ball-milling with diamond powder and a second part of copper powder to obtain Cu-Ti-diamond mixed powder;
(3) hot-pressing and sintering: carrying out sectional sintering on the Cu-Ti-diamond mixed powder in a hot pressing sintering furnace or a hot isostatic pressing sintering furnace in vacuum, inert gas or reducing atmosphere, and cooling to obtain a finished copper-based composite material;
in the step sintering, the sintering temperature of the first step is 800-950 ℃, the sintering pressure is 20-200MPa, the heat preservation time is 0.5-1h, the sintering temperature of the second step is 1050-1300 ℃, the sintering pressure is 200-600MPa, and the heat preservation time is 1-5 h.
2. The diamond @ TiC reinforced high-strength conductive copper-based composite material as claimed in claim 1, wherein in the step (1), the particle size of the titanium powder is 5-300 μm, the purity is greater than 99%, the particle size of the diamond powder is 0.5-50 μm, the purity is greater than 99%, the particle size of the copper powder is 1-400 μm, and the purity is greater than 99%.
3. The diamond @ TiC reinforced high-strength conductive copper-based composite material of claim 1, wherein the mass ratio of the titanium powder to the first portion of copper powder in the step (2) is 1: 0.5-6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110441817.2A CN113512661B (en) | 2021-04-23 | 2021-04-23 | Diamond @ TiC enhanced high-strength conductive copper-based composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110441817.2A CN113512661B (en) | 2021-04-23 | 2021-04-23 | Diamond @ TiC enhanced high-strength conductive copper-based composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113512661A CN113512661A (en) | 2021-10-19 |
| CN113512661B true CN113512661B (en) | 2022-04-29 |
Family
ID=78061565
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110441817.2A Active CN113512661B (en) | 2021-04-23 | 2021-04-23 | Diamond @ TiC enhanced high-strength conductive copper-based composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113512661B (en) |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101139515B (en) * | 2007-05-18 | 2010-08-18 | 中南大学 | High heat-conductive diamond-copper composite encapsulating material and method for making same |
| CN103898344B (en) * | 2012-12-24 | 2016-03-30 | 北京有色金属研究总院 | A kind of preparation method of copper base diamond matrix composite materials |
| CN104060117A (en) * | 2014-07-08 | 2014-09-24 | 武汉理工大学 | Preparation method for diamond/copper-based composite material |
| CN105506345B (en) * | 2015-12-15 | 2018-03-23 | 北京有色金属与稀土应用研究所 | High heat-conductive diamond/copper composite encapsulating material and preparation method thereof |
| CN108179302B (en) * | 2018-01-30 | 2019-12-10 | 哈尔滨工业大学 | preparation method of high-thermal-conductivity diamond/copper composite material |
| US20200010929A1 (en) * | 2018-07-08 | 2020-01-09 | Ariel Scientific Innovations Ltd. | Copper-based substances with nanomaterials |
| CN109182802B (en) * | 2018-11-12 | 2021-11-05 | 华北电力大学（保定） | Preparation method of carbon material reinforced copper/aluminum-based composite material |
| CN112609115B (en) * | 2020-11-30 | 2022-09-13 | 北京有色金属与稀土应用研究所 | Diamond/copper heat sink material for electronic packaging and preparation method thereof |
-
2021
- 2021-04-23 CN CN202110441817.2A patent/CN113512661B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN113512661A (en) | 2021-10-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104711443B (en) | A kind of graphene/copper composite material and preparation method thereof | |
| CN107012355B (en) | A kind of preparation method of single-layer graphene reinforced aluminum matrix composites | |
| CN107022691B (en) | A method of graphene reinforced aluminum matrix composites are prepared by raw material of multi-layer graphene microplate | |
| CN100436616C (en) | Preparation method of near fully densificated high W or Mo content W-Cu or Mo-Cu composite material | |
| CN110157932B (en) | Preparation method of graphene modified copper-based electrical contact material based on in-situ synthesis | |
| CN101728279B (en) | Preparation method of high-performance diamond reinforced Al-matrix electronic packaging composite material | |
| CN111500892A (en) | Preparation method of large-size flaky diamond/copper composite material with ultrahigh thermal conductivity | |
| CN110144508B (en) | Two-stage powder metallurgy preparation method of tungsten/steel bimetal collar material | |
| CN112981164B (en) | Preparation method of diamond reinforced metal matrix composite material with high reliability and high thermal conductivity | |
| CN113881875B (en) | Three-dimensional framework structure metal reinforced aluminum matrix composite material and preparation method thereof | |
| CN114309596B (en) | Preparation method of high-heat-conductivity surface-metallized diamond/copper composite substrate | |
| CN108149059A (en) | A kind of TiC enhances the preparation method of copper-based electric contact composite material | |
| CN112974774B (en) | Silver-based composite material and preparation method thereof | |
| CN101942591A (en) | Method for fast preparing molybdenum-copper alloy | |
| CN103302294A (en) | Method for preparing nano Cu coated SiC/Cu based composite by powder metallurgic method | |
| Dong et al. | W–Cu system: synthesis, modification, and applications | |
| CN114525438B (en) | Tungsten copper composite material and preparation method thereof | |
| CN107841669B (en) | High-thermal-conductivity active composite packaging material and preparation method thereof | |
| CN111118324A (en) | Preparation method of TiC reinforced copper-based composite material added with coupling agent | |
| CN100363131C (en) | Method for preparing grain-size-contrdlable superfine crystallite tungsten and tungsten-copper composite material | |
| CN113512661B (en) | Diamond @ TiC enhanced high-strength conductive copper-based composite material and preparation method thereof | |
| CN110453126A (en) | A kind of diamond-metal-based compound Heat Conduction Material and preparation method thereof | |
| Wang et al. | Thermal conducting property of SiCp-reinforced copper matrix composites by hot pressing | |
| CN116287833A (en) | Preparation method of in-situ authigenic two-dimensional carbide dispersion strengthening and toughening molybdenum alloy | |
| CN110257664B (en) | Copper-based composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |